HRID1702612

反应详情

EQUATION

反应方程式

HRID 1702612 的结构方程式

PROCEDURE

实验过程

A mixture of 16.7 g. of 5-isopropoxyanthranilic acid, 10.0 g. of 2-chloro-5-cyanopyridine and 0.01 g. of potassium iodide in 30 ml. of triglyme was heated to a bath temperature of 150° overnight under a stream of argon. On cooling, the mixture was triturated with ethanol and water. A gummy solid was collected, dissolved in hot ethyl acetate, filtered and the filtrate was evaporated to give 8.4 g. of crude product (38% yield). Two recrystallizations of this solid from dimethylformamide-acetic acid-water give pure 8-cyano-2-isopropoxy-11-oxo-11H-pyrido[2,1-b]quinazoline, mp 234°-236°.

WORKUP

后处理

  1. additionA mixture of 16.7 g
  2. temperatureOn cooling
  3. customthe mixture was triturated with ethanol and water
  4. customA gummy solid was collected
  5. dissolutiondissolved in hot ethyl acetate
  6. filtrationfiltered
  7. customthe filtrate was evaporated
  8. customto give 8.4 g
  9. customTwo recrystallizations of this solid from dimethylformamide-acetic acid-water